반응 #439636

반응 방정식

6-methyl isatoic anhydride

acid chloride

2-Methyl-6-(trifluoromethyl)-3-pyridinecarbonyl chloride

pyridine

→

title compound

8-Methyl-2-[2-methyl-6-(trifluoromethyl)-3-pyridinyl]-4H-3,1-benzoxazine

반응 조건

후처리

1. 1
   기타the solvent was removed under reduced pressure
2. 2
   기타Excess pyridine was removed by azeotrope with toluene
3. 3
   workup.ADDITIONEther was added
4. 4
   기타the resulting brown solid was removed by filtration
5. 5
   workup.ADDITIONThe solid was taken up in a mixture of aqueous sodium bicarbonate and chloroform
6. 6
   건조the chloroform extracts were dried over magnesium sulfate
7. 7
   기타evaporated
8. 8
   기타Excess pyridine was again removed by azeotrope with toluene

실험 절차

A mixture of the 6-methyl isatoic anhydride (3.92 g, 22.1 mmol) and the acid chloride from Step A (5.45 g, 24.3 mmol) was heated at reflux in pyridine for 16 hours. The dark brown solution was cooled to room temperature and the solvent was removed under reduced pressure. Excess pyridine was removed by azeotrope with toluene. Ether was added and the resulting brown solid was removed by filtration. The solid was taken up in a mixture of aqueous sodium bicarbonate and chloroform, the chloroform extracts were dried over magnesium sulfate and evaporated. Excess pyridine was again removed by azeotrope with toluene to afford 5.1 g of the title compound as a brown solid.

출처